EP2612706B1 - Procédé de production d'hydrogène - Google Patents

Procédé de production d'hydrogène Download PDF

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Publication number
EP2612706B1
EP2612706B1 EP10856674.6A EP10856674A EP2612706B1 EP 2612706 B1 EP2612706 B1 EP 2612706B1 EP 10856674 A EP10856674 A EP 10856674A EP 2612706 B1 EP2612706 B1 EP 2612706B1
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Prior art keywords
ammonia
metal
oxide
catalyst
temperature
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German (de)
English (en)
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EP2612706A4 (fr
EP2612706A1 (fr
Inventor
Sadao Araki
Susumu Hikazudani
Takuma Mori
Akira Taniguchi
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Hitachi Zosen Corp
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Hitachi Zosen Corp
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
    • C01B3/047—Decomposition of ammonia
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/14—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of germanium, tin or lead
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/20—Vanadium, niobium or tantalum
    • B01J23/22—Vanadium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/24—Chromium, molybdenum or tungsten
    • B01J23/26—Chromium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/32—Manganese, technetium or rhenium
    • B01J23/34—Manganese
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/56—Platinum group metals
    • B01J23/63—Platinum group metals with rare earths or actinides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/66—Silver or gold
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0201—Impregnation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/03—Precipitation; Co-precipitation
    • B01J37/031—Precipitation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Definitions

  • the present invention relates to a process for producing hydrogen by carrying out oxidation/decomposition of ammonia in the presence of ammonia oxidation/decomposition catalyst comprising a support composed of an oxidizable and reducible metal oxide and a catalytically active metal supported theron.
  • a temperature drop in the case where 100 % of ammonia is decomposed is about 900°C.
  • a gas temperature in a downstream region of the catalyst layer at, for example, 350°C or higher, it is necessary to set an inlet gas temperature at 1,250°C or higher, and hence, such is not practical.
  • heat was conventionally supplied from the outside.
  • a rate of heat transfer is slower than the reaction rate, in order to obtain a sufficient rate of heat transfer, an area of heat-transfer surface must be made large, and it is difficult to achieve compactification of the apparatus.
  • the reactions of the equations (1) and (2) are made to take place in the same reaction tube, it is possible to compensate heat for the endothermic reaction of the equation (I) by heat generated in the equation (II).
  • the oxygen amount in the equation (II) the temperature of a catalyst layer can be controlled. For example, in the case where the temperature of a supply gas pre-heated by heat exchange of waste heat of the engine exhaust gas fluctuates, it becomes possible to stably produce hydrogen.
  • Patent Document 1 proposes a multilayered ammonia oxidation catalyst composed of a refractory metal oxide, a layer of platinum disposed on this refractory metal oxide, and a layer of vanadia disposed on this platinum.
  • the working temperature of this catalyst is about 200°C, and if the temperature is not higher than this temperature, the oxidation reaction cannot be allowed to proceed, and hence, it is necessary to increase the gas temperature to about 200°C by an electric heater or the like.
  • Patent Document 2 proposes an ammonia oxidation catalyst composed of an oxide of at least one element selected from cerium and praseodymium, an oxide of at least one element selected from non-variable valency rare earth elements including yttrium, and an oxide of cobalt.
  • Patent Document 3 proposes an ammonia oxidation catalyst containing filaments substantially composed of platinum and rhodium and if desired, palladium, the filaments having a platinum coating.
  • these patent documents have the same problem as that in Patent Document 1, too.
  • Patent documents 4 and 5 disclose an ammonia deposition catalyst as a catalyst for decomposing ammonia into nitrogen and hydrogen which is obtained by depositing a compound of an iron group metal on a support composed of metal oxides such as ceria, lanthanum oxide, etc. then treating the compound with reducing gas at a temperature from 300°C to 800°C. Furthermore patent documents 4 and 5 disclose when two or more metal oxides are used, composite oxide, a solid solution of ceria and zirkonia, or the like may be preferred.
  • Patent document 6 discloses an ammonia decomposing catalyst which is obtained by supporting at least one kind of the platinum group elements selected from the group consisting of VIII-X elements to a metal oxide of which acid strength is -5,6 or above.
  • Patent document 7 discloses a decomposing method of ammonia from a gas containing ammonia which is brought into contact with a catalyst for decomposition of ammonia.
  • the catalyst is obtained by depositing platinum as active metal on a carrier which consists of crystalline silicate having a specified chemical composition.
  • Patent document 8 discloses an ammonia oxidation catalyst which comprises a carrier containing a silica-alumina composite oxide and platinum carried on a carrier.
  • the catalyst has a higher average weight ratio of silica/alumina on the partical surface layer of the composite oxide when that of the whole partical.
  • An object of the present invention is to provide an ammonia oxidation/decomposition catalyst capable of overcoming the foregoing problems.
  • the present invention is concerned with a process for producing hydrogen by carrying out oxidation/decomposition of ammonia in the presence of an ammonia oxidation/decomposition catalyst comprising a support composed of an oxidizable and reducible metal oxide and a catalytically active metal supported thereon.
  • the metal oxide may be a composite oxide.
  • the metal oxide is preferably a rare earth metal oxide.
  • the oxidizable and reducible metal oxide refers to a metal capable of being reversibly converted between an oxidized state and a reduced state.
  • the oxidizable and reducible metal oxide include rare earth metal oxides such as cerium oxide, lanthanum oxide, samarium oxide, etc.
  • the oxidizable and reducible metal oxide may also be a composite oxide of a rare earth metal and at least one metal selected from the group consisting of magnesium, titanium, zirconium, yttrium, aluminum, silicon, cobalt, iron, and gallium.
  • it may also be a composition oxide of a rare earth metal and at least two metals selected from the group consisting of magnesium, titanium, zirconium, yttrium, aluminum, silicon, cobalt, iron, and gallium.
  • the catalytically active metal which is supported on the support is preferably at least one metal selected from the group consisting of a metal belonging to the Group VIII, such as ruthenium, platinum, rhodium, palladium, iron, cobalt, nickel, etc., tin, copper, silver, manganese, chromium, and vanadium.
  • a metal belonging to the Group VIII such as ruthenium, platinum, rhodium, palladium, iron, cobalt, nickel, etc., tin, copper, silver, manganese, chromium, and vanadium.
  • the ammonia oxidation/decomposition catalyst according to the present invention is provided for an ammonia oxidation/decomposition reaction after a heat treatment in a hydrogen gas stream at 200°C or higher, preferably from 200 to 700°C, and especially preferably from 200 to 600°C and subsequently, reduction of a part or the whole of the metal oxide constituting the support.
  • the reduction treatment of the ammonia oxidation/decomposition catalyst may be carried out either prior to or after charging in the same catalyst reactor.
  • the support of the ammonia oxidation/decomposition catalyst can be, for example, prepared in the following method.
  • a method of supporting the catalytically active metal on the thus prepared support to obtain the ammonia oxidation/decomposition catalyst is, for example, as follows.
  • the above-described ammonia oxidation/decomposition catalyst is charged in a reactor, and reduction of the support is carried out in a hydrogen gas stream while heating at, for example, 600°C. Subsequently, when the resultant is brought into contact with ammonia and air at ordinary temperature, the support in a reduced state first reacts with oxygen to generate oxidation heat, and the temperature of the catalyst layer is increased in a moment. Once the temperature of the catalyst layer is increased to a temperature (200°C) at which ammonia and oxygen react with each other, the ammonia oxidation reaction proceeds autonomously after that according to the above-described equation (II). The heat generated in this exothermic reaction (II) is used in the course of decomposing ammonia in the presence of the catalytically active metal according to the above-described equation (I), thereby producing hydrogen.
  • the ammonia oxidation/decomposition catalyst comprising a support composed of an oxidizable and reducible metal oxide and a catalytically active metal supported thereon according to the present invention at ordinary temperature
  • the support in a reduced state first reacts with oxygen to generate oxidation heat, and the temperature of the catalyst layer is increased in a moment.
  • the temperature of the catalyst layer is increased to a temperature at which ammonia and oxygen react with each other, the ammonia oxidation reaction proceeds autonomously after that.
  • the heat generated in this exothermic reaction (II) is used in the course of decomposing ammonia in the presence of the catalytically active metal according to the above-described equation (I), thereby producing hydrogen. According to this, the need for pre-heating by an electric heater or the like can be eliminated, and the production costs of hydrogen can be reduced.
  • the ammonia oxidation/decomposition catalyst was charged in a charge amount shown in Table 1 in a flow-type reactor and then heated in a hydrogen gas stream at 600°C for 2 hours, thereby subjecting the catalyst to a reduction treatment. After cooling to ordinary temperature, an ammonia gas and air were supplied to this reactor. The supply amount of ammonia was kept constant at 100 NL/min, and the supply amount of air was set at air/NH 3 of 1. An outlet temperature of the ammonia oxidation/decomposition catalyst and a generation amount of hydrogen were measured. The measurement of the generation amount of hydrogen was carried out by measuring the gas concentration by a mass analyzer.
  • Table 1 Example Catalyst and charge amount Oxidation rate of ammonia Yield of hydrogen Supported metal Charge amount 1 Cerium oxide Ruthenium 40 mL 100 40 2 Cerium oxide Ruthenium 150 mL 100 70 3 Lanthanum oxide Ruthenium 40 mL 100 32 4 Samarium oxide Ruthenium 40 mL 100 30 5 Ce-Zr composite oxide Ruthenium 40 mL 100 43 6 Ce-Ti composite oxide Ruthenium 40 mL 100 38 7 Ce-Mg composite oxide Ruthenium 40 mL 100 38 8 Ce-Zr-Al composite oxide Ruthenium 40 mL 100 45 9 Ce-Zr-Si composite oxide Ruthenium 40 mL 100 42 10 Cerium oxide Platinum 40 mL 100 18 11 Lanthanum oxide Platin um 40 mL 100 8 12 Samarium oxide Platinum 40 mL 100 6 13 Cerium oxide Platinum 40 mL 100 18 14 Cerium oxide Rhodium 40 mL 100 35 15 Cerium oxide Palladium 40 mL 100 15 16 Ce
  • the ammonia oxidation reaction can be started up at ordinary temperature, hydrogen can be obtained in a high yield upon decomposition of ammonia without adopting pre-heating by an electric heater or the like, and a decrease in the cost of production of hydrogen can be achieved.
  • ammonia oxidation/decomposition catalyst By using the ammonia oxidation/decomposition catalyst according to the present invention, the need for pre-heating by an electric heater or the like can be eliminated, and the production costs of hydrogen can be reduced.

Claims (1)

  1. Un procédé de production d'hydrogène par oxydation/décomposition d'ammoniac en présence d'un catalyseur d'oxydation/décomposition d'ammoniac comprenant un support composé d'un oxyde métallique oxydable et réductible et d'un métal catalytiquement actif sur celui-ci,
    l'oxyde de métal étant un oxyde de métal des terres rares qui est l'oxyde de cérium, l'oxyde de lanthane ou l'oxyde de samarium, ou un oxyde composite d'un métal des terres rares et d'au moins un métal choisi dans le groupe constitué par le magnésium, le titane, le zirconium, l'yttrium, l'aluminium, le silicium, le cobalt, le fer, le gallium,
    le métal catalytiquement actif étant au moins un métal choisi dans le groupe constitué par un métal appartenant au groupe VIII, l'étain, le cuivre, l'argent, le manganèse, le chrome et le vanadium, et
    le flux d'hydrogène étant chauffé à 200°C ou plus,
    le procédé comprenant
    réduire le support en chauffant dans un courant d'hydrogène, et
    la mise en contact de l'ammoniac et de l'air avec le catalyseur à température ordinaire,
    de telle sorte que le support réduit réagisse avec l'oxygène pour générer de la chaleur d'oxydation, la température de la couche de catalyseur soit augmentée en un instant à une température à laquelle l'ammoniac réagit avec l'oxygène, et la chaleur générée par l'oxydation d'ammoniac selon l'équation suivante :

            NH3 + 3/4O2 -> 1/2N2 + 3/2H2O (réaction exothermique)

    soit utilisé pour décomposer l'ammoniac en présence du catalyseur selon l'équation suivante :

            2NH3 -> 3H2 + N2 (réaction endothermique)

    produisant ainsi de l'hydrogène.
EP10856674.6A 2010-08-31 2010-08-31 Procédé de production d'hydrogène Active EP2612706B1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2010/064799 WO2012029122A1 (fr) 2010-08-31 2010-08-31 Catalyseur d'oxydation/décomposition d'ammoniac

Publications (3)

Publication Number Publication Date
EP2612706A1 EP2612706A1 (fr) 2013-07-10
EP2612706A4 EP2612706A4 (fr) 2016-11-02
EP2612706B1 true EP2612706B1 (fr) 2019-10-30

Family

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EP10856674.6A Active EP2612706B1 (fr) 2010-08-31 2010-08-31 Procédé de production d'hydrogène

Country Status (5)

Country Link
US (1) US9580309B2 (fr)
EP (1) EP2612706B1 (fr)
CN (1) CN103079693B (fr)
DK (1) DK2612706T3 (fr)
WO (1) WO2012029122A1 (fr)

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EP2612706A1 (fr) 2013-07-10
US20130156687A1 (en) 2013-06-20
DK2612706T3 (da) 2020-01-02
WO2012029122A1 (fr) 2012-03-08
CN103079693A (zh) 2013-05-01
CN103079693B (zh) 2014-12-17
US9580309B2 (en) 2017-02-28

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